Bromine → 5-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-one

HRID 598081노트

반응식

HRID 598081 반응식
[CH3:1][S:2][C:3]1[NH:8][C:7](=[O:9])[CH:6]=[CH:5][N:4]=1.[Br:10]Br>C(O)(=O)C>[Br:10][C:6]1[C:7](=[O:9])[NH:8][C:3]([S:2][CH3:1])=[N:4][CH:5]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 798232-(Methylthio)-1H-pyrimidin-4-one

생성물 1

HCID 2405655-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-one수율 45.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

To a solution containing 2.0 g (14 mmol) of 2-(methylthio)pyrimidin-4(3H)-one in 10 ml of acetic acid under a nitrogen atmosphere was added 1.04 ml (14 mmol) of bromine in 2 ml acetic acid. The reaction was allowed to stir at room temperature for 30 min. The precipitated product was filtered, washed with acetic acid and suspended in hot acetic acid. To this suspension was added 0.2 ml bromine in 1 ml acetic acid. The product was collected, washed with acetic acid and recrystallized from ethanol to yield 1.4 g (45%) of product.

후처리

  1. filtrationThe precipitated product was filtered
  2. washwashed with acetic acid
  3. additionTo this suspension was added 0.2 ml bromine in 1 ml acetic acid
  4. customThe product was collected
  5. washwashed with acetic acid
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-b4e8dd88e8b74127887858907dba5968
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897607B2

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